反応 #93024

反応方程式

benzhydryl 7-phenylacetamido-3-formyl-2-cephem-4-carboxylate

triphenylphosphine

carbon tetrachloride

ethyl acetate

→

benzhydryl 7-phenylacetamido-3-(2,2-dichlorovinyl)-2-cephem-4-carboxylate

溶媒

N,N-dimethylacetamide

反応条件

後処理

1. 1
   温度After being cooled
2. 2
   その他the resulting precipitates
3. 3
   ろ過were filtered off
4. 4
   その他the filtrate was evaporated in vacuo
5. 5
   その他The residue was purified by column chromatography on silica gel

実験手順

Zinc powder (78.4 g) was added to a solution of benzhydryl 7-phenylacetamido-3-formyl-2-cephem-4-carboxylate (102.4 g) and triphenylphosphine (367.2 g) in a mixture of carbon tetrachloride (800 ml) and N,N-dimethylacetamide (200 ml) at ambient temperature and the mixture was stirred at 60° C. for 30 minutes. After being cooled, the mixture was added to ethyl acetate (20 l) and the resulting precipitates were filtered off and the filtrate was evaporated in vacuo. The residue was purified by column chromatography on silica gel to give benzhydryl 7-phenylacetamido-3-(2,2-dichlorovinyl)-2-cephem-4-carboxylate (15.26 g).

出典